反应详情

温度

45 °C

A suspension of the the product from Example 8, Step 1 (0.190 g, 0.700 mmol) in ethanol (3.5 mL) was saturated with ammonia, capped, and heated to 45° C. for three hours. The mixture was cooled, concentrated, and triturated with diethylether. Crude product was recrystallized from dimethylformamide/water to give 0.129 g (77%) of the title compound as a pale yellow solid, one-eighth hydrate: mp 215° C.; 1H NMR (DMSO-d6): δ9.87 (s, 1H), 9.34 (s, 1H), 8.60 (d, 1H), 7.40-8.60 (broad signal, NH2), 8.02 (d, 1H), 7.86 (d, 1H), 7.77 (d, 1H), 7.68 (t, 1H). IR (KBr): 3200, 1800, 1690, 1650 cm-1 ; MS (m/z) 240(MH+).

1. customcapped
2. temperatureThe mixture was cooled
3. concentrationconcentrated
4. customtriturated with diethylether
5. customCrude product was recrystallized from dimethylformamide/water